CN101944367A - Magnetic recording disk composition with lubricator is than the manufacture method of assay method and magnetic recording disk - Google Patents

Magnetic recording disk composition with lubricator is than the manufacture method of assay method and magnetic recording disk Download PDF

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Publication number
CN101944367A
CN101944367A CN2010102130016A CN201010213001A CN101944367A CN 101944367 A CN101944367 A CN 101944367A CN 2010102130016 A CN2010102130016 A CN 2010102130016A CN 201010213001 A CN201010213001 A CN 201010213001A CN 101944367 A CN101944367 A CN 101944367A
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Prior art keywords
composition
magnetic recording
recording disk
end group
mentioned
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铃木宏太
下川贡一
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WD Media Singapore Pte Ltd
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Hoya Corp
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    • G—PHYSICS
    • G11—INFORMATION STORAGE
    • G11B—INFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
    • G11B5/00—Recording by magnetisation or demagnetisation of a record carrier; Reproducing by magnetic means; Record carriers therefor
    • G11B5/84—Processes or apparatus specially adapted for manufacturing record carriers
    • G11B5/8408—Processes or apparatus specially adapted for manufacturing record carriers protecting the magnetic layer
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M107/00—Lubricating compositions characterised by the base-material being a macromolecular compound
    • C10M107/38—Lubricating compositions characterised by the base-material being a macromolecular compound containing halogen
    • G—PHYSICS
    • G11—INFORMATION STORAGE
    • G11B—INFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
    • G11B5/00—Recording by magnetisation or demagnetisation of a record carrier; Reproducing by magnetic means; Record carriers therefor
    • G11B5/62—Record carriers characterised by the selection of the material
    • G11B5/72—Protective coatings, e.g. anti-static or antifriction
    • G11B5/725—Protective coatings, e.g. anti-static or antifriction containing a lubricant, e.g. organic compounds
    • G11B5/7253—Fluorocarbon lubricant
    • G11B5/7257—Perfluoropolyether lubricant
    • G—PHYSICS
    • G11—INFORMATION STORAGE
    • G11B—INFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
    • G11B5/00—Recording by magnetisation or demagnetisation of a record carrier; Reproducing by magnetic means; Record carriers therefor
    • G11B5/74—Record carriers characterised by the form, e.g. sheet shaped to wrap around a drum
    • G11B5/82—Disk carriers
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/08—Resistance to extreme temperature
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/14—Electric or magnetic purposes
    • C10N2040/18—Electric or magnetic purposes in connection with recordings on magnetic tape or disc

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Lubricants (AREA)
  • Magnetic Record Carriers (AREA)
  • Manufacturing Of Magnetic Record Carriers (AREA)

Abstract

The invention provides a kind of magnetic recording disk composition with lubricator than assay method, it is characterized in that, by adopting the nuclear magnetic resonance optical spectroscopy, carry out with 19F is the 1st assay method of object, to analyze raw material, in above-mentioned raw materials, introduces functional group and changes the structure of end group, thus the material that acquires change, then by adopting the nuclear magnetic resonance optical spectroscopy to carry out with relevant with the material that changes 1H is the 2nd assay method of object, to determine the composition ratio of lubricant.The present invention also provides a kind of manufacture method of the magnetic recording disk composition with lubricator of claim 1 than the magnetic recording disk of assay method acquisition of passing through to adopt.

Description

Magnetic recording disk composition with lubricator is than the manufacture method of assay method and magnetic recording disk
And the manufacture method of magnetic recording disk
The application is dividing an application of No. the 200680036127.2nd, Chinese patent application, and the original bill international application no is PCT/JP/2006/319371, and the original bill international filing date is on September 28th, 2006.
Technical field
The present invention relates to the manufacture method of magnetic recording disk composition with lubricator than assay method and magnetic recording disk.In more detail, the material technology that relates to lubricating layer.
Background technology
Magnetic recording disk at least by magnetosphere, protective seam and lubricating layer according to this sequential laminating on non-magnetic substrate and constitute, wherein, lubricating layer has relax the function of impacting when magnetic recording disk contacts with magnetic head.Magnetic recording disk drive unit for HDD being representative is accompanied by recording capacity and obviously increases, and the gap between magnetic recording disk and the magnetic head can further narrow down.Especially, by adopting LUL (load/unload) mode, the floatation volume of magnetic head has the tendency of further reduction, even people require also can stably carry out work under the condition of so extremely low floatation volume below the 10nm.
Promptly, under this condition, at first, because the magnetic recording disk in the high speed rotating contacts intermittently with magnetic head, the part that is contacted reaches a high temperature (flash of light temperature) owing to friction sometimes, and therefore, people require lubricating layer to have thermotolerance, even under this hot conditions, decomposition and evaporation etc. can not take place owing to being heated in lubricating layer yet.
In addition, if magnetic recording disk high speed rotating, what is called migration (migration) phenomenon that lubricating layer moves will take place, thereby the thickness that can make lubricating layer becomes inhomogeneous easily, in this state, when carrying out LUL when operation, often be created in magnetic head when outer circumferential side enters, to fly-problem of viscous (fly stiction) fault.So-called flight-viscous fault is meant that magnetic head causes floating the fault that posture or floatation volume change when floating flight, be attended by irregular regeneration and export.In addition, according to different occasions, floating in-flight, magnetic recording disk contacts with magnetic head, tends to cause that magnetic head damages the fault of disc surface (head crash).Therefore, people also require lubricating layer to be difficult for taking place transport phenomena.
At this requirement, people often use the FOMBLINE Z base lubricant of the Solvaysolexis corporate system with superior heat resistance, long-time stability as the lubricant that forms the magnetic recording disk lubricating layer.In addition, in order further to improve the performance of this lubricant, need from this based composition, remove impurity or carry out various refining for suitableization of distribution that makes molecular weight.In addition, when making with extra care, used to use weight-average molecular weight (Mw), number-average molecular weight (Mn) as parameter (with reference to patent documentation 1).
Patent documentation 1: the spy opens the 2004-319058 communique
Summary of the invention
The problem that invention will solve
But, there are such problem in weight-average molecular weight or number-average molecular weight, promptly, owing to can not directly, specifically determine the composition of lubricating layer, therefore, can not correctly estimate properties of lubricants, particularly can not correctly estimate the transport phenomena that becomes the reason of flight-viscous fault whether easily.Therefore, though as long as determine lubricant from molecular structure and quantitative aspect,, if employing method is in the past analyzed lubricating layer with the nuclear magnetic resonance optical spectroscopy, as shown in Figure 3, from methylene (CH 2-) the peak will with from hydroxyl (peak area OH) overlaps, therefore can not from molecular structure and quantitatively the aspect determine lubricant, this is the problem that exists.
In view of above problem, problem of the present invention is, provides a kind of and can try hard to reduce the floatation volume of magnetic head by determining lubricant from molecular structure and quantitative aspect, can bring into play the magnetic recording disk and the manufacture method thereof of high reliability again.
Be used to solve the means of problem
In order to solve above-mentioned problem, the inventor has proposed to be suitable for adopting the nuclear magnetic resonance optical spectroscopy to analyze the method for lubricant, carry out the various lubricants that various variations form by the ratio of components of estimating by per-fluoro polyether compound, constituted the lubricant that can solve above-mentioned problem with various different end groups.
Promptly; the present invention be at least by magnetosphere, protective seam and lubricating layer by this sequential laminating to non-magnetic substrate and the magnetic recording disk that constitutes; it is characterized in that; in this magnetic recording disk; the serve as reasons per-fluoro polyether compound of following chemical formula (changing 1) expression of the major component that constitutes the lubricant of above-mentioned lubricating layer, this per-fluoro polyether compound contains: end group X is by X 1The 1st composition of expression, end group X are by X 2The 2nd composition of expression and end group X are by X 3The 3rd composition of expression, and, press above-mentioned the 1st composition, above-mentioned the 2nd composition and the content of above-mentioned the 3rd composition in this per-fluoro polyether compound that the analysis of nuclear magnetic resonance optical spectroscopy obtains, count in molar ratio, be following ratio:
Above-mentioned the 1st composition: above-mentioned the 2nd composition: above-mentioned the 3rd composition=71～73: 15～17: 11～13
[changing 1]
X-OCH 2CF 2-(CF 2O) m(C 2F 4O) n-CF 2OCH 2O-X
m，n＝9～11
The 1st composition: X=X 1=CH 2CH (OH) CH 2OH
The 2nd composition: X=X 2=CH 2CH (OH) CH 2OCH 2CH (OH) CH 2OH
The 3rd composition: X=X 3=H.
In the present invention, press above-mentioned the 1st composition, above-mentioned the 2nd composition and the total content of above-mentioned the 3rd composition in above-mentioned per-fluoro polyether compound that the analysis of nuclear magnetic resonance optical spectroscopy obtains, meter is preferably more than 99.0% in molar ratio.
The present invention be at least by magnetosphere, protective seam and lubricating layer by this sequential laminating to non-magnetic substrate and the magnetic recording disk that constitutes; it is characterized in that; in this magnetic recording disk; the major component that constitutes the lubricant of above-mentioned lubricating layer is the per-fluoro polyether compound by above-mentioned chemical formula (changing 1) expression, and this per-fluoro polyether compound contains: end group X is by X 1The 1st composition of expression, end group X are by X 2The 2nd composition of expression, end group X are by X 3The 3rd composition of expression, and press above-mentioned the 1st composition, above-mentioned the 2nd composition and the total content of above-mentioned the 3rd composition in above-mentioned per-fluoro polyether compound that the analysis of nuclear magnetic resonance optical spectroscopy obtains, meter is more than 99.0% in molar ratio.
In the present invention, also contain in following chemical formula (changing 2), end group X is by X 4The 4th composition of expression, end group X are by X 5The 5th composition of expression, and press above-mentioned the 4th composition and the total content of above-mentioned the 5th composition in above-mentioned per-fluoro polyether compound that the analysis of nuclear magnetic resonance optical spectroscopy obtains, meter is preferably below 1.0% in molar ratio,
[changing 2]
X-OCH 2CF 2-(CF 2O) m(C 2F 4O) n-CF 2OCH 2O-X
m，n＝9～11
The 1st composition: X=X 1=CH 2CH (OH) CH 2OH
The 2nd composition: X=X 2=CH 2CH (OH) CH 2OCH 2CH (OH) CH 2OH
The 3rd composition: X=X 3=H
The 4th composition: X=X 4=CF 3
The 5th composition: X=X 5=CF 2Cl.
In the present invention, also contain end group X in the above-mentioned chemical formula (change 2) by X when above-mentioned lubricant 4The 4th composition of expression and end group X are by X 5During the 5th composition of expression, press the content that the analysis of nuclear magnetic resonance optical spectroscopy obtains, preferably above-mentioned the 4th composition lacks than above-mentioned the 5th composition.
In the present invention, above-mentioned protective seam is made of for example carbon class material.
The manufacture method of magnetic recording disk of the present invention, the preferred use by lubricant is carried out the above-mentioned lubricant that molecular distillation obtains with starting material forms above-mentioned lubricating layer.
The invention effect
According to the present invention, determined the end group of contained per-fluoro polyether compound the lubricant from structure and quantitative aspect, therefore, can clearly determine properties of lubricants.Therefore, in the present invention, can positively obtain thermotolerance height and the difficult lubricant that becomes the transport phenomena of flight-viscous failure cause.Therefore, according to the present invention, the floatation volume that can provide a class can realize reducing magnetic head can be brought into play the magnetic recording disk of high reliability again.
Description of drawings
(A) of Fig. 1, (B) are respectively planimetric map and the summary sectional view that magnetic recording disk is shown.
Fig. 2 illustrates the simple key diagram that constitutes of molecular distillation apparatus.
Fig. 3 is that illustrating direct is the key diagram that object comes analytical sample is carried out nuclear magnetic resonance result that spectrum analysis obtains with 1H.
Symbol description
1 magnetic recording disk
11 non-magnetic substrates
12 magnetospheres
13 protective seams
14 lubricating layers
Embodiment
Below, with reference to the description of drawings embodiments of the present invention.
[formation of magnetic recording disk]
(A) of Fig. 1, (B) are respectively planimetric map and the summary sectional view that magnetic recording disk is shown.
As shown in these figures, the magnetic recording disk 1 of this programme have a kind of by bottom (not shown), the structure that on the surface of the circular non-magnetic substrate 11 that has center pit 111, forms according to this sequential laminating of the lubricating layer 14 that adopts magnetosphere 12 that the DC magnetron sputtering system forms, protective seam 13 that using plasma CVD method forms and employing infusion process to form.Non-magnetic substrate 11 is made of chemically reinforced glass such as for example sillico aluminate glass.Protective seam 13 is that the hydrogenated carbon (diamond-like-carbon [diamond-like-carbonl) of 5nm constitutes by for example thickness, is bearing the function that improves abrasion performance and protect magnetosphere 12.Lubricating layer 14 is that the so thin macromolecular material of 1.2nm constitutes by for example thickness, the function of the impact when bearing mitigation and contacting with magnetic head.In order to adopt infusion process to form this lubricating layer 14; the magnetic recording base-board for plate that forms protective seam 13 is impregnated into that lubricant by regulation is dissolved in organic solvent and in the test solution that forms; then; heat-treat with its taking-up and to it, thereby lubricant is adhered securely as lubricating layer 14.
[making of lubricating layer]
Fig. 2 illustrates the simple key diagram that constitutes of molecular distillation apparatus.In this programme, lubricant as the lubricating layer 14 that is used for magnetic recording disk 1, can make by the multiple per-fluoro polyether compound that contains different end group according to the ratio of components of stipulating separately, carry out various tests at the magnetic recording disk that uses this lubricant to form lubricating layer 14.In this programme, when making this lubricant, the lubricant of the FOMBLINE Z system (trade name) of use Solvaysolexis corporate system etc. will use as lubricant behind this raw material refining as starting material.As process for purification, can adopt supercritical extraction method, gel permeation chromatography (GPC) method, molecularly distilled etc., in this programme, use distilling apparatus shown in Figure 2 that starting material are carried out molecular distillation, make various lubricants thus.
, record when adopting following nuclear magnetic resonance optical spectroscopy to analyze, above-mentioned raw-material major component is by the per-fluoro polyether compound of following chemical formula (changing 3) expression, as this per-fluoro polyether compound, contains end group X by X according to following ratio of components herein 1The 1st composition (single adduct) of expression, end group X are by X 2The 2nd composition (diadduct) of expression, end group X are by X 3The 3rd composition of expression, end group X are by X 4The 4th composition of expression and end group X are by X 5The 5th composition of expression.
The 1st composition=71.9%
The 2nd composition=10.5%
The 3rd composition=15.0%
The 4th composition=1.4%
The 5th composition=1.2%
[changing 3]
X-OCH 2CF 2-(CF 2O) m(C 2F 4O) n-CF 2OCH 2O-X
m，n＝9～11
The 1st composition: X=X 1=CH 2CH (OH) CH 2OH
The 2nd composition: X=X 2=CH 2CH (OH) CH 2OCH 2CH (OH) CH 2OH
The 3rd composition: X=X 3=H
The 4th composition: X=X 4=CF 3
The 5th composition: X=X 5=CF 2Cl
In addition, above-mentioned starting material have attribute shown below:
Number-average molecular weight (Mn)=2326.50
Corresponding these raw-material mean molecular weight=627.06 of 1-OH of average every existence base institute
In average each molecule-average=3.71 of OH
(C on the main chain 2F 4O)/(CF 2O) ratio=0.89.
In order to use molecular distillation apparatus shown in Figure 2 300 to make with extra care starting material, at first, in charging bottle 31, add starting material.Though molecular distillation not necessarily will carry out under reduced pressure atmosphere,, wish in the reduced pressure atmosphere of regulation, to carry out in the occasion of the starting material that contain macromolecule component being carried out molecular distillation.This is because if do not carry out molecular distillation in reduced pressure atmosphere, the molecule of the composition that has then gasified and the raising of the frequency of other molecular collisions thus, have hindered starting material to be liquefied in interior distance in mean free path.Therefore, after in charging bottle 31, dropping into material, with carrying out exhaust in 42 pairs of devices of exhaust apparatus, so that reach the decompression degree of regulation.The decompression degree preference of this moment is as being 1 * 10 -2Pa～1 * 10 -3About Pa, perhaps in this high vacuum below value.The decompression degree can be measured with vacuum meter 40.Should illustrate that the reduced pressure atmosphere in can use device is in advance to the contained processing that outgas such as foreign gas in the material in the charging bottle 31.At this moment, contained foreign gas etc. flow into exhaust apparatus 42 1 sides by pipe arrangement 44 in the starting material, and a part wherein accumulates in the low boilers cold-trap 39.In addition, as required, also can heat with the starting material in 32 pairs of charging bottles of mantle heater 31 of charging bottle.
After in device, reaching the decompression degree of regulation, starting material are flow into distillation this pipe 35 from charging bottle 31.Flow into the raw-material amount (inlet amount) of distillation this pipe 35 from charging bottle 31, the switching amount of valve 35 that can be by being arranged on charging bottle 31 lower ends is controlled.Generally, the inlet amount about 1～30g/ divides is suitable.If inlet amount is very few, then the distillation need take a long time, and if inlet amount is too much, then distillation efficiency often reduces.
Flow into the starting material in distillation this pipe 35, be configured in the temperature that this pipe of distillation 35 cylindraceous this pipe of distillation mantle heater 36 on every side is heated to regulation.In the present embodiment, heating-up temperature is for making the temperature of starting material gasification at least.Should illustrate, control to raw-material heating-up temperature, can be undertaken by the temperature of this pipe of control distillation mantle heater 36, also can measure the raw-material actual heating-up temperature of distilling in this pipe 35 by the thermometer that is arranged in this pipe of distillation 35.
In addition, on the length direction in distillation this pipe 35, the magnetic coupling stirrer 33 that setting is made of the slide (wiper) of for example fluororesin system, by stirrer control enclosure 34, the rotational speed about making this slide by 20～100rpm is rotated on certain orientation.By the rotation of this slide, starting material are film like on the tube wall surface of distillation this pipe 35, and gasification easily becomes.The starting material that gasified contact with cooling stick 46 in being arranged on this pipe of distillation 35 and are liquefied, and accumulate in the flask 38 of reception distillate.In the cooling stick 46, import chilled water, and discharge from escape hole 46b from the inflow entrance 46a of lower end.Should illustrate, not gasify and accumulate in residue in the flask 37 that receives residue, can utilize this pipe of distillation mantle heater 36 to change heating-up temperature, and then it is put in the charging bottle 31, distill repeatedly.In addition, more than shown in operation, control by operation board 43.
When using this molecular distillation apparatus 300 preparation lubricants, at first, starting material are put in the charging bottle 31 in the molecular distillation apparatus 300, will be decompressed to 1 * 10 in the molecular distillation apparatus 300 with exhaust apparatus 42 then -3Pa.In addition, the reduced pressure atmosphere in the use device is in advance to the contained processing that outgas fully such as foreign gas in the starting material in the charging bottle 31.Then, flow into distillation this pipe 35 from charging bottle 31 with certain inlet amount.At this moment, the slide in this pipe of distillation 35 is driven with predetermined rotational speed.Should illustrate that the temperature of distilling in this pipe 35 is 180 ℃ that equate with the design temperature of mantle heater 36.Then, in the flask 38 that receives distillate, obtain 180 ℃ distillate, thereby obtain lubricant.Should illustrate that making with extra care in the toilet of above lubricant carried out.Atmosphere gas in the employed toilet is the clean atmosphere gas of a kind of cleaniliness classs 6 than Japanese Industrial Standards (JIS) B9920 regulation.
Should illustrate; in order to use this lubricant to form lubricating layer 14; lubricant is scattered among Vertrel XF (trade name) as the Mitsui Du Pont fluorine chemistry corporate system of fluorous solvent etc.; form test solution; the magnetic recording base-board for plate that forms protective seam 13 is impregnated in the above-mentioned test solution; then it is heat-treated,, thereby form lubricating layer 14 so that lubricant is adhered on the magnetic recording base-board for plate securely.
[adopting the analytical approach of nuclear magnetic resonance optical spectroscopy]
Therefore the nuclear magnetic resonance optical spectroscopy is based on when material applies magnetic field, and the spin states that atomic nucleus had is split into 2 kinds of spin states, can analyze by the radiated wave that irradiation is equivalent to the energy difference between spin states.Herein, therefore the energy difference between spin states, for the peak that obtains, can belong to each atom in the molecule owing to reflect the residing electronic environment of its proton nuclei (chemical environment), thereby determines the amount of each atom in its molecule.Therefore, the structure of analyzing molecules at length.
According to the nuclear magnetic resonance optical spectroscopy, the nucleic that can measure is the whole nucleic that have nuclear spin in theory, as its typical example, 1H, 13C, 19F, 31P is arranged.Wherein, be object with 1H, as shown in Figure 3, because from methylene (CH 2-) the peak and from hydroxyl therefore (peak area OH) is overlapped, is difficult to determine lubricant from structure and quantitative two aspects.Therefore, in this programme,, adopt the nuclear magnetic resonance optical spectroscopy to analyze lubricant by with following 2 kinds of methods and usefulness.
At first, the 1st kind of method is to be the method for object with 19F, when adopting this method that starting material are analyzed, the result as shown below,
The composition that chemical shift (relative value ppm) is corresponding
-52.1 belong to the peak of main chain
-53.7 belong to the peak of main chain
-55.4 belong to the peak of main chain
-89.1 belong to the peak of main chain
-90.7 belong to the peak of main chain
-125.8 belong to the peak of main chain
-129.7 belong to the peak of main chain
The composition that chemical shift (relative value ppm) is corresponding
-81.3 belong to the peak of the end group of the 3rd composition
-83.3 belong to the peak of the end group of the 3rd composition
-56.3 belong to the peak of the end group of the 4th composition
-58.0 belong to the peak of the end group of the 4th composition
-27.7 belong to the peak of the end group of the 5th composition
-29.3 belong to the peak of the end group of the 5th composition
-74.5 belong to the peak of the end group of the 5th composition
-78.0 belong to the peak base at peak of the end group of the 1st, 2 compositions
Overlapped
-80.0 belong to the peak base at peak of the end group of the 1st, 2 compositions
Overlapped
The signal of each composition has appearred in the chemical shift with regulation.Herein, the peak area ratio of each signal just becomes the existence ratio of the fluorine element in each composition, therefore, can determine the shape of end group, and can be by recently definite molecular weight of main chain and end group.
Secondly, the 2nd kind of method is with the method for 1H as object, in advance by with starting material with agent treated to wherein introducing functional group, change the structure of its end group thus, analyze then.Its result can obtain showing the signal with the corresponding composition of following chemical shift (relative value ppm):
5.5 belong to the peak of the 1st composition
5.3 belong to the peak of the 2nd composition.
Therefore, can determine the ratio of the 1st composition and the 2 one-tenth branches.
[formation of lubricating layer]
To adopt the analysis result of this analytical approach and use the test findings of the magnetic recording disk 1 of each lubricant to compare, if the composition of the lubricant of the best is represented with the analysis result that adopts the nuclear magnetic resonance optical spectroscopy, then in per-fluoro polyether compound, contain end group X by X according to following ratio of components (mol ratio in the per-fluoro polyether compound) by above-mentioned chemical formula (changing 3) expression 1The 1st composition (single adduct) of expression, end group X are by X 2The 2nd composition (diadduct) of expression, end group X are by X 3The 3rd composition of expression, end group X are by X 4The 4th composition of expression and end group X are by X 5The 5th composition of expression:
The 1st composition=71.7%
The 2nd composition=15.7%
The 3rd composition=11.7%
The 4th composition=0.3%
The 5th composition=0.6%.
In addition, this lubricant has attribute shown below:
Number-average molecular weight (Mn)=2630.12
1-OH of average every existence base institute is mean molecular weight=656.31 of this lubricant accordingly
In average each molecule-average=4.01 of OH
(C on the main chain 2F 4O)/(CF 2O) ratio=0.91.
In addition, even be set in 10nm when following from floatation volume with magnetic head, can guarantee that also magnetic recording head 1 has the viewpoint consideration of enough reliabilities, when stipulating the ratio of components of each composition, then when adopting the nuclear magnetic resonance optical spectroscopy to analyze, can obtain the content of the 1st composition, the 2nd composition and the 3rd composition, count in molar ratio, preferably in per-fluoro polyether compound, contain the result of following ratio:
71～73∶15～17∶11～13。
Promptly; in per-fluoro polyether compound; in the per-fluoro polyether compound of pure modification; contain the compound that diol compound, three alcoholic compounds, tetrol compound etc. have various end-group structures; the degree of alcohol modification; that is, the hydroxyl number difference of bonding on the end group of perfluor ether main chain, the greasy property of lubrication molecule then can be different with the adhesion to protective seam 13.Therefore, as long as limit the ratio of various pure modified compounds such as diol compound, three alcoholic compounds, tetrol compound, just can positively determine the greasy property of lubrication molecule and to the adhesion of protective seam 13.
In addition, even be set at 10nm when following in floatation volume with magnetic head, from guaranteeing that magnetic recording head 1 has the viewpoint consideration of enough reliabilities, when determining the total content of the 1st composition, the 2nd composition and the 3rd composition that employing nuclear magnetic resonance optical spectroscopy records when analyzing, can obtain total content and count the result who is preferably more than 99.0% in molar ratio.That is, state raw-material occasion in the use, when adopting the nuclear magnetic resonance optical spectroscopy to analyze, can obtain its total content and count the result who is preferably below 1.0% in molar ratio the 4th composition that contained and the 5th composition.
And then, can obtain the result that the 4th composition preferably lacks than the 5th composition.Its reason can think, and is as the 4th composition and the 5th composition of impurity contained in the lubricant, at high temperature relatively poor to the degree of the facilitation that decomposition rose of lubricant.
(other embodiment)
Should illustrate, formation (shape, size and configuration relation) about among the figure that uses when the present embodiment is described only is shown schematically in and is appreciated that and implements degree of the present invention, and, for the composition (material) in numerical value and each formation, but only illustrate.Therefore, the present invention is not limited to the embodiment of above explanation, the change that can suit in the scope that does not deviate from technological thought shown in the claim.

Claims (3)

1. magnetic recording disk composition with lubricator is characterized in that than assay method,
By adopting the nuclear magnetic resonance optical spectroscopy, carry out with 19F is the 1st assay method of object, with the analysis raw material,
In above-mentioned raw materials, introduce functional group and change the structure of end group, thus the material that acquires change,
Then by adopting the nuclear magnetic resonance optical spectroscopy to carry out with relevant with the material that changes 1H is the 2nd assay method of object, to determine the composition ratio of lubricant.
2. the manufacture method of magnetic recording disk has adopted the assay method of claim 1, it is characterized in that,
Preparation contains the lubricant starting material of per-fluoro polyether compound,
By super critical extraction, gel permeation chromatography or molecularly distilled, this lubricant is made with extra care with starting material, make the result who measures according to the method for claim 1 drop in the scope that is predetermined to be proportion by subtraction, obtain magnetic recording disk with lubricator,
Use this magnetic recording disk with lubricator, on the protective seam of magnetic recording base-board for plate, form lubricating layer.
3. the manufacture method of the described magnetic recording disk of claim 2 is characterized in that,
Above-mentioned magnetic recording disk with lubricator contains the per-fluoro polyether compound of following chemical formula (changing 1) expression as major component,
This per-fluoro polyether compound contains: end group X is by X 1The 1st composition of expression, end group X are by X 2The 2nd composition of expression and end group X are by X 3The 3rd composition of expression,
Measure the composition ratio of above-mentioned the 1st composition, above-mentioned the 2nd composition and above-mentioned the 3rd composition by the method for claim 1,
[changing 1]
X-OCH 2CF 2-(CF 2O) m(C 2F 4O) n-CF 2OCH 2O-X
m，n＝9～11
The 1st composition: X=X 1=CH 2CH (OH) CH 2OH
The 2nd composition: X=X 2=CH 2CH (OH) CH 2OCH 2CH (OH) CH 2OH
The 3rd composition: X=X 3=H
CN2010102130016A 2005-09-30 2006-09-28 Magnetic recording disk composition with lubricator is than the manufacture method of assay method and magnetic recording disk Pending CN101944367A (en)

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